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NASA NTRS2004

Effects of Initial Powder Size on the Mechanical Properties and Microstructure of As-Extruded GRCop-84

GRCop-84 was developed to meet the mechanical and thermal property requirements for advanced regeneratively cooled rocket engine main combustion chamber liners. It is a ternary Cu- Cr-Nb alloy having approximately 8 at% Cr and 4 at% Nb. The chromium and niobium constituents combine to form 14 vol% Cr2Nb, the strengthening phase. The alloy is made by producing GRCop-84 powder through gas atomization and consolidating the powder using extrusion, hot isostatic pressing (HIP) or vacuum plasma spraying (VPS). GRCop-84 has been selected by Rocketdyne, Ratt & Wlutney and Aerojet for use in their next generation of rocket engines. GRCop-84 demonstrates favorable mechanical and thermal properties at elevated temperatures. Compared to NARloy-Z, the currently used inaterial in the Space Shuttle, GRCop-84 has approximately twice the yield strength, 10-1000 times the creep life, and 1.5-2.5 times the low cycle fatigue life. The thermal expansion of GRCop-84 is 7515% less than NARloy-Z which minimizes thermally induced stresses. The thermal conductivity of the two alloys is comparable at low temperature but NARloy-Z has a 20-50 W/mK thermal conductivity advantage at typical rocket engine hot wall temperatures. GRCop-84 is also much more microstructurally stable than NARloy-Z which translates into better long term stability of mechanical properties. Previous research into metal alloys fabricated by means of powder metallurgy (PM), has demonstrated that initial powder size can affect the microstructural development and mechanical properties of such materials. Grain size, strength, ductility, size of second phases, etc., have all been shown to vary with starting powder size in PM-alloys. This work focuses on characterizing the effect of varying starting powder size on the microstructural evolution and mechanical properties of as- extruded GRCop-84. Tensile tests and constant load creep tests were performed on extrusions of four powder meshes: +140 mesh (great3er than l05 micron powder size), -140 mesh (less than or equal to 105 microns), -140 plus or minus 270 (53 - 105 microns), and - 270 mesh (less than or equal to 53 microns). Samples were tested in tension at room temperature and at 500 C (932 F). Creep tests were performed under vacuum at 500 C using a stress of 111 MPa (16.1 ksi). The fracture surfaces of selected samples from both tests were studied using a Scanning Electron Microscope (SEM). The as-extruded materials were also studied, using both optical microscopy and SEM analysis, to characterize changes within the microstructure.

Okoro, Chika L.↗

NASA NTRS2000

Contaminated Solar Array Handrail Samples Retrieved From Mir Analyzed

In January 1998 during the shuttle STS 89 mission, an eight-section Russian solar array panel was retrieved after more than 10 years of exposure to the orbital space environment on Mir. The array was deployed June 16, 1987, and removed on November 3, 1997. It had been actively used as a source of electrical power for 8 years. This operational array had been located on the Mir core module, located directly above the Kvant-2 module. Its retrieval provided a unique opportunity to study the effects of the low-Earth-orbit environment on a functional solar array. The intact solar array underwent scientific inspections and preliminary tests by a joint team of U.S. and Russian investigators to evaluate the effects of long-term space exposure. Upon initial examination, significant contamination was observed over most components of the array. One panel, panel 8, was provided to the U.S. scientists for further evaluation. As part of the U.S. investigations, two solar array handrail samples from panel 8 were evaluated for contamination at the NASA Glenn Research Center at Lewis Field. One is a section of a rigid handrail, and the other is a section of woven fabric tape that was overwrapped around a flexible handhold. Both the flexible handhold woven fabric and the rigid handrail were significantly darkened after 10 years of space exposure. They were evaluated with optical microscopy, field emission scanning electron microscopy (FESEM), and energy-dispersive spectroscopy. Solar absorptance and room-temperature emittance values also were obtained. The returned contaminated solar array segment is very similar in design to the solar arrays being supplied by the Russians for the International Space Station. Therefore, it was desirable to determine what the contaminants on various surfaces are and what the sources of the contamination were.

deGroh, Kim K.↗

NASA NTRS2004

Active Metal Brazing of Carbon-Carbon Composites to Titanium

The Ti-metal/C-C composite joints were formed by reactive brazing with three commercial brazes, namely, Cu-ABA, TiCuNi, and TiCuSil. The joint microstructures were examined using optical microscopy, and scanning electron microscopy (SEM) coupled with energy dispersive spectrometry (EDS). The results of the microstructure analysis indicate solute redistribution across the joint which led to good wetting, spreading, and metallurgical bond formation via interdiffusion.

Singh, M.↗

NASA NTRS2004

Reactive Brazing of Carbon-Carbon Composites to Titanium

The Ti-metal/C-C composite joints were formed by reactive brazing with three commercial brazes, namely, Cu-ABA, TiCuNi, and TiCuSil. The joint microstructures were examined using optical microscopy, and scanning electron microscopy (SEM) coupled with energy dispersive spectrometry (EDS). The results of the microstructure analysis indicate solute redistribution across the joint and possible metallurgical bond formation via interdiffusion, which led to good wetting and spreading.

Shpargel, Tarah↗

NASA NTRS1990

Failure Morphologies of Cyclically Oxidized ZrO2-Based Thermal Barrier Coatings

Plasma-sprayed thermal barrier coatings (TBC s) were thermal cycle tested in air at 1163 C until spallation of the top coat. Each thermal cycle consisted of a 45 minute exposure at the elevated temperature followed by a 15 minute cool to ambient temperature. The TBC s consisted of a ZrO2-based top coat containing various amounts of Y2O3, and/or Yb2O3, Gd2O3, and Nd2O3 applied by air plasma spraying and an MCrAlY bond coat applied by low pressure plasma spraying. The substrate was a single-crystal, Ni-based superalloy. The time to failure of the top coat varied from tens to hundreds of thermal cycles based on composition and spray parameters. The bond coat/top coat interface morphology and sample cross sections were examined by SEM and optical microscopy. The failure morphology following the cyclic oxidation testing will be discussed in relationship to the properties of the ceramic top coats.

Nesbit, James A.↗

NASA NTRS2006

Active Metal Brazing and Characterization of Brazed Joints in Titanium to Carbon-Carbon Composites

The Ti-metal/C-C composite joints were formed by reactive brazing with three commercial brazes, namely, Cu-ABA, TiCuNi, and TiCuSiI. The joint microstructures were examined using optical microscopy and scanning electron microscopy (SEM) coupled with energy dispersive spectrometry (EDS). The results of the microstructure analysis indicate solute redistribution across the joint and possible metallurgical bond formation via interdiffusion, which led to good wetting and spreading. A tube-on-plate tensile test was used to evaluate joint strength of Ti-tube/ C-C composite joints. The load-carrying ability was greatest for the Cu-ABA braze joint structures. This system appeared to have the best braze spreading which resulted in a larger braze/C-C composite bonded area compared to the other two braze materials. Also, joint loadcarrying ability was found to be higher for joint structures where the fiber tows in the outer ply of the C-C composite were aligned perpendicular to the tube axis when compared to the case where fiber tows were aligned parallel to the tube axis.

Singh, M.↗

NASA NTRS2006

Active Metal Brazing and Adhesive Bonding of Titanium to C/C Composites for Heat Rejection System

Robust assembly and integration technologies are critically needed for the manufacturing of heat rejection system (HRS) components for current and future space exploration missions. Active metal brazing and adhesive bonding technologies are being assessed for the bonding of titanium to high conductivity Carbon-Carbon composite sub components in various shapes and sizes. Currently a number of different silver and copper based active metal brazes and adhesive compositions are being evaluated. The joint microstructures were examined using optical microscopy, and scanning electron microscopy (SEM) coupled with energy dispersive spectrometry (EDS). Several mechanical tests have been employed to ascertain the effectiveness of different brazing and adhesive approaches in tension and in shear that are both simple and representative of the actual system and relatively straightforward in analysis. The results of these mechanical tests along with the fractographic analysis will be discussed. In addition, advantages, technical issues and concerns in using different bonding approaches will also be presented.

Singh, M.↗

NASA NTRS2006

Novel Nanolaminates for Aerospace Applications

Nanolaminate manufacturing (NLM) is a new way of developing materials whose properties can far exceed those of homogeneous materials. Traditional alloys, composites and bulk laminates tend to average the properties of the materials from which they were made. With nanostructured materials, the high density of interfaces between dissimilar materials results in novel material properties. For example, materials made -from alternating nanoscale layers of metals and oxides have exhibited thermal conductivities far below those of the oxides themselves. Also, metallic nanolaminates can have peak strengths 100 times lager than the bulk constituent metals. Recent work at MSFC has focused on the development of nickel/aluminum oxide (Ni/Al2O3)) nanolaminates. Ni/Al2O3 nanolaminates are expected to have better strength, creep and fatigue resistance, oxygen compatibility, and corrosion resistance than the traditional metal-matrix composites of this material, which has been used in a variety of aerospace applications. A chemical vapor deposition (CW) system has been developed and optimized for the deposition of nanolaminates. Nanolaminates with layer thicknesses between 10 and 300 nm have been successfully grown and characterization has included scanning electron microscopy (SEM) and atomic force microscopy (AFM) Nanolaminates have a large variety of potential applications. They can be tailored to have both very small and anisotropic thermal conductivities and are promising as thermal coatings for both rock$ engine components and aerobraking structures. They also have the potential to be used in aerospace applications where strength at high temperatures, corrosion resistance or resistance to hydrogen embrittlement is important. Both CVD and magnetron sputtering facilities are available for the deposition of nanolayered materials. Characterization equipment includes SEM, AFM, X-ray diffraction, transmission electron microscopy, optical profilometry, and mechanical tensile pull testing.

Volz, Martin↗

NASA NTRS2007

Brazing of Stainless Steel to Yttria-Stabilized Zirconia Using Gold-Based Brazes for Solid Oxide Fuel Cell Applications

Two gold-base active metal brazes (gold-ABA and gold-ABA-V) were evaluated for oxidation resistance to 850 C, and used to join yttria-stabilized zirconia (YSZ) to a corrosion-resistant ferritic stainless steel for possible use in solid oxide fuel cells. Thermogravimetric analysis and optical microscopy and scanning electron microscopy coupled with energy-dispersive spectroscopy were used to evaluate the braze oxidation behavior, and microstructure and composition of the YSZ/braze/steel joints. Both gold-ABA and gold-ABA-V exhibited nearly linear oxidation kinetics at 850 C, with gold-ABA-V showing faster oxidation than gold-ABA. Both brazes produced metallurgically sound YSZ/steel joints due to chemical interactions of Ti and V with the YSZ and steel substrates.

Singh, M.↗

NASA NTRS2007

In-Plane Cracking Behavior and Ultimate Strength for 2D Woven and Braided Melt-Infiltrated SiC/SiC Composites Tensile Loaded in Off-Axis Fiber Directions

The tensile mechanical properties of ceramic matrix composites (CMC) in directions off the primary axes of the reinforcing fibers are important for architectural design of CMC components that are subjected to multi-axial stress states. In this study, 2D-woven melt-infiltrated (MI) SiC/SiC composite panels with balanced fiber content in the 0 degree and 90 degree directions were tensile loaded in-plane in the 0 degree direction and at 45 degree to this direction. In addition, a 2D triaxially-braided MI composite panel with balanced fiber content in the plus or minus 67 degree bias directions and reduced fiber content in the axial direction was tensile loaded perpendicular to the axial direction tows (i.e., 23 degrees from the bias fibers). Stress-strain behavior, acoustic emission, and optical microscopy were used to quantify stress-dependent matrix cracking and ultimate strength in the panels. It was observed that both off-axis loaded panels displayed higher composite onset stresses for through-thickness matrix cracking than the 2D-woven 0/90 panels loaded in the primary 0 degree direction. These improvements for off-axis cracking strength can in part be attributed to higher effective fiber fractions in the loading direction, which in turn reduces internal stresses on critical matrix flaws for a given composite stress. Also for the 0/90 panel loaded in the 45 degree direction, an improved distribution of matrix flaws existed due to the absence of fiber tows perpendicular to the loading direction. In addition, for the +67/0/-67 braided panel, the axial tows perpendicular to the loading direction were not only low in volume fraction, but were also were well separated from one another. Both off-axis oriented panels also showed relatively good ultimate tensile strength when compared to other off-axis oriented composites in the literature, both on an absolute strength basis as well as when normalized by the average fiber strength within the composites. Initial implications are discussed for constituent and architecture design to improve the directional cracking of SiC/SiC CMC components with MI matrices.

Morscher, Gregory N.↗

NASA NTRS2007

Oxidation Through Coating Cracks of SiC-Protected Carbon/Carbon

The oxidation of SiC-protected carbon/carbon through machined slots and naturally occurring craze cracks in the SiC was studied. The slot and crack geometries were characterized, and the subsurface oxidation of the carbon/carbon substrate at temperatures of 1000 to 1300 C in air was assessed using weight change, x-ray computed tomography, and optical microscopy of sections. Rate constants were derived from these measurements and compared with a two-step diffusion control model of carbon oxidation. Oxidation kinetic measurements on both the specimens with machined slots and with naturally occurring craze cracks showed good agreement with the model.

Jacobson, Nathan S.↗

NASA NTRS2007

Oxidation Through Coating Cracks of SiC-Protected Carbon/Carbon

Jacobson, Nathan S.↗

NASA NTRS2005

Aligned Single Wall Carbon Nanotube Polymer Composites Using an Electric Field

While high shear alignment has been shown to improve the mechanical properties of single wall carbon nanotubes (SWNT)-polymer composites, it is difficult to control and often results in degradation of the electrical and dielectric properties of the composite. Here, we report a novel method to actively align SWNTs in a polymer matrix, which allows for control over the degree of alignment of SWNTs without the side effects of shear alignment. In this process, SWNTs are aligned via field-induced dipolar interactions among the nanotubes under an AC electric field in a liquid matrix followed by immobilization by photopolymerization while maintaining the electric field. Alignment of SWNTs was controlled as a function of magnitude, frequency, and application time of the applied electric field. The degree of SWNT alignment was assessed using optical microscopy and polarized Raman spectroscopy and the morphology of the aligned nanocomposites was investigated by high resolution scanning electron microscopy. The structure of the field induced aligned SWNTs is intrinsically different from that of shear aligned SWNTs. In the present work, SWNTs are not only aligned along the field, but also migrate laterally to form thick, aligned SWNT percolative columns between the electrodes. The actively aligned SWNTs amplify the electrical and dielectric properties in addition to improving the mechanical properties of the composite. All of these properties of the aligned nanocomposites exhibited anisotropic characteristics, which were controllable by tuning the applied field conditions.

Park, Cheol↗

NASA NTRS2008

Oxidation Through Coating Cracks of SiC-Protected Carbon/Carbon

Jacobson, Nathan S.↗

NASA NTRS2008

Oxygen Plasma Modification of Poss-Coated Kapton(Registered TradeMark) HN Films

The surface energy of a material depends on both surface composition and topographic features. In an effort to modify the surface topography of Kapton(Registered TradeMark) HN film, organic solutions of a polyhedral oligomeric silsesquioxane, octakis(dimethylsilyloxy)silsesquioxane (POSS), were spray-coated onto the Kapton(Registered TradeMark) HN surface. Prior to POSS application, the Kapton(Registered TradeMark) HN film was activated by exposure to radio frequency (RF)-generated oxygen plasma. After POSS deposition and solvent evaporation, the films were exposed to various durations of RF-generated oxygen plasma to create a topographically rich surface. The modified films were characterized using optical microscopy, attenuated total reflection infrared (ATR-IR) spectroscopy, and high-resolution scanning electron microscopy (HRSEM). The physical properties of the modified films will be presented.

Wohl, C. J.↗

NASA NTRS2008

Effect of Weld Tool Geometry on Friction Stir Welded Ti-6Al-4V

In this study, flat 0.250" thick Ti-6Al-4V panels were friction stir welded (FSWed) using weld tools with tapered pins. The five different pin geometries of the weld tools included: 0 degree (straight cylinder), 15 degree, 30 degree, 45 degree, and 60 degree angles on the frustum. All weld tools had a smooth 7 degree concave shoulder and were made from microwave sintered tungsten carbide. For each weld tool geometry, the FSW process parameters were optimized to eliminate internal defects. All the welds were produced in position control with a 2.5 degree lead angle using a butt joint configuration for the panels. The process parameters of spindle rpm and travel speed were varied, altering the hot working conditions imparted to the workpiece. Load cells on the FSWing machine allowed for the torque, the plunge force, and the plow force to be recorded during welding. Resulting mechanical properties were evaluated from tensile tests results of the FSWjoints. Variations in the material flow were investigated by use of microstructural analysis including optical microscopy (OM), scanning electron microscopy (SEM), and orientation image mapping (aIM).

Querin, Joseph A.↗

NASA NTRS2008

Microstructural Evolution in Friction Stir Welding of Ti-6Al-4V

Friction stir welding (FSW) is a thermo-mechanical process that utilizes a nonconsumable rotating pin tool to consolidate a weld joint. In the conventional FSW process, the pin tool is responsible for generating both the heat required to soften the material and the forces necessary to deform and combine the weld seam. As such, the geometry of the pin tool is important to the quality of the weld and the process parameters required to produce the weld. Because the geometry of the pin tool is limitless, a reduced set of pin tools was formed to systematically study their effect on the weldment with respect to mechanical properties and resultant microstructure. In this study 0deg, 15deg, 30deg, 45deg, and 60deg tapered, microwave sintered, tungsten carbide (WC) pin tools were used to FSW Ti-6Al-4V. Transverse sections of the weld were used to test for mechanical properties and to document the microstructure using optical microscopy. X-ray diffraction (XRD) was also used to characterize the microstructure in the welds. FSW results for the 45deg and 60deg pin tools are reported in this paper.

Rubisoff, H.↗

NASA NTRS2009

Investigating the Effects of Pin Tool Design on Friction Stir Welded Ti-6Al-4V

Friction stir welding (FSWing), a solid state joining technique, uses a non-consumable rotating pin tool to thermomechanically join materials. Heating of the weldment caused by friction and deformation is a function of the interaction between the pin tool and the work piece. Therefore, the geometry of the pin tool is in part responsible for the resulting microstructure and mechanical properties. In this study microwave sintered tungsten carbide (WC) pin tools with tapers and flats were used to FSW Ti-6Al-4V. Transverse sections of welds were mechanically tested, and the microstructure was characterized using optical microscopy (OM) and scanning election microscopy (SEM). X-ray diffraction (XRD) and electron back-scatter diffraction (EBSD) were used to characterize the texture within the welds produced from the different pin tool designs.

Rubisoff, H. A.↗